Method for semi-quantitative determination of ethyl carbamate through thin layer chromatography

A urethane and thin-layer chromatography technique, which is applied in the field of urethane content detection, can solve the problems of high professional and technical requirements for personnel, complicated pretreatment methods, expensive equipment and other problems, and achieves that the reaction conditions are easy to control and easy to use. Operation, low cost effect

Inactive Publication Date: 2014-11-12
SOUTH CHINA UNIV OF TECH
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  • Description
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Problems solved by technology

The above detection methods have high accuracy, but there are disadvantages such as expensive instruments and e

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  • Method for semi-quantitative determination of ethyl carbamate through thin layer chromatography

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Embodiment 1

[0028] (1) Take out the thin-layer silica gel plate 5cm×10cm, activate it in an oven at 110°C for half an hour, and put it in a desiccator for later use;

[0029] (2) Prepare developer (methyl tert-butyl ether: petroleum ether: methanol = 5:7:3 (volume ratio), pour it into a double-slot thin-layer chromatography development cylinder after stirring, and let it stand for at least half an hour to make the saturation;

[0030] (3) Prepare fluorescent derivative solution, cinnamaldehyde 160μL, acetone 40ml, phosphoric acid 2.4ml in a small beaker, stir for later use;

[0031] (4) Take out the thin-layer board, spot the sample at 1cm from the lower end of the thin-layer board, and mark with a pencil 2cm from the upper end of the thin-layer board as the unfolding front, and place the sample. The first sample point is 20μL urethane standard solution (5mg / L, 40% ethanol aqueous solution), and the second point is placed at a distance of 2cm from the first point, and the sample is 20μL ...

Embodiment 2

[0036] (1) Take out the thin-layer silica gel plate 5cm×10cm, activate it in an oven at 110°C for half an hour, and put it in a desiccator for later use;

[0037](2) Prepare developing agent methyl tert-butyl ether: petroleum ether: methanol = 5:7:3 (volume ratio), pour it into a thin layer developing tank after stirring, and let it stand for at least half an hour to make it saturated;

[0038] (3) Prepare fluorescent derivative solution, cinnamaldehyde 160μL, acetone 40ml, phosphoric acid 2.4ml in a small beaker, stir for later use;

[0039] (4) Take out the thin-layer board, spot the sample at 1cm from the lower end of the thin-layer board, and mark with a pencil 2cm from the upper end of the thin-layer board as the unfolding front, and place the sample. The first sample point is 20μL urethane standard solution (5mg / L, 40% ethanol aqueous solution), and the second point is placed at a distance of 2cm from the first point, and the sample is 20μL urethane standard solution (10...

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Abstract

The invention provides a method for semi-quantitative determination of ethyl carbamate through a thin layer chromatography. According to the method, mixed liquor of cinnamyl aldehyde and phosphoric acid is used as a fluorescence derivating agent, mixed liquor of methyl tertiary butyl ether, petroleum ether and methyl alcohol is used as mobile phase developing solvent, a chromatographic sheet is used as an immobile phase, after the ethyl carbamate developed by a thin layer is reacted with the fluorescence derivating agent, accordingly, green fluorescent spots can be observed at the position of 365 nm through a common ultraviolet analysis meter, the Rf value is 0.85, and the lowest drug loading capacity of a thin layer plate is 50 ng of ethyl carbamate. According to the limiting standard of 5 mg/L ethyl carbamate in wine, 2.5 mg/L EC can be detected directly, and the sample application amount of the thin layer plate is generally 20 microliters maximally. The method is small in number of needed samples, rapid, high in sensitivity, simple in step, small in number of needed equipment and easy to operate. In accordance with the principle, a rapid test kit can be researched and developed, and the method is used for rapidly detecting the ethyl carbamate in alcoholic beverages and fermented food.

Description

technical field [0001] The invention relates to a method for detecting the content of ethyl carbamate, in particular to a method for semi-quantitatively measuring the content of ethyl carbamate by thin-layer chromatography. Background technique [0002] Ethyl Carbamate (EC) is a compound with potential carcinogenic effects, which can lead to diseases such as liver cancer, skin cancer, lung cancer and lymph cancer, and is an accompanying product of fermented food and alcoholic beverages. EC was confirmed as a carcinogen as early as 1943. In 1976, Ough (Ough C S. Ethyl carbamate in fermented beverages and foods. Ⅱ. Possible formation of ethyl carbamate from diethyl dicarbonate addition to wine [J]. Agric FoodChem, 1976, 24(2): 328-331.) was found in Alcoholic beverages contain EC. Studies have shown that EC is a multi-site carcinogen in rodents and that ethanol (alcohol) promotes its carcinogenicity. In 2007, the International Cancer Institute changed the carcinogenic toxic...

Claims

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Application Information

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IPC IPC(8): G01N30/90
Inventor 黄惠华王浩周端刘智钧黄秋婷
Owner SOUTH CHINA UNIV OF TECH
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